CN103276469B - Production method of concrete reinforced and toughened PVA (polyvinyl alcohol) fiber - Google Patents
Production method of concrete reinforced and toughened PVA (polyvinyl alcohol) fiber Download PDFInfo
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Abstract
The invention discloses a production method of concrete reinforced and toughened PVA (polyvinyl alcohol) fiber. The production method comprises the following steps of: (1) dissolving PVA; (2) carrying out primary filtering; (3) defoaming; (4) carrying out secondary filtering; (5) spinning; (6) carrying out wet stretching by using a guide roller; (7) neutralizing and decrosslinking; (8) carrying out hot and damp stretching; (9) carrying out water washing; (10) oiling; (11) drying; (12) preheating; (13) carrying out dry heat stretching; (14) carrying out surface treatment on fiber; (15) drying; (16) winding; and (17) cutting off and packaging. The concrete reinforced and toughened PVA produced by using the production method has the advantages of high tensile strength, elasticity modulus, elongation at break, length-diameter ratio and interfacial friction bonding strength and high production process.
Description
Technical field
The present invention relates to concrete PVA fiber art, refer more particularly to the production method of the enhancing of a kind of concrete, toughness reinforcing PVA fiber.
Background technology
Cement-based material is current the most large manufactured construction materials, is developed so far the history of existing more than 170 years.Intensity is the main performance index of concrete as important feature material always, and concrete high-strength is concrete research and development striving direction for many years.But the intrinsic weakness-tension of concrete, bending resistance, shock resistance, antiknock and poor toughness etc. but still limit giving full play to of its advantage, and improving constantly along with concrete strength, this weakness is also more outstanding.It has been generally acknowledged that, concrete strength is higher, and its toughness is poorer, and fragility is higher, structure ductility and anti-crack ability more not enough, to the potential safety hazard that structural seismic performance brings.Therefore, many scholars constantly explore the method and access improving the above-mentioned performance of concrete for a long time.Fibre reinforced concrete is exactly one of Recent study and most widely used important channel.It is plateau modulus short fiber reinforced concrete that current fibre reinforced concrete mainly contains two kinds: one, and it represents fiber is steel fibre; Two is low-elasticity-modulus amount short fiber reinforced concrete, and it represents fiber is polypropylene and nylon fiber.But these two kinds of fibers only play humidification to concrete, poor to concrete cracking resistance, toughening effect.
Polyvinyl alcohol (PVA) fiber reinforcement, toughness reinforcing cement-base composite material (being called for short PVA-ECC), for base material with cement mortar, mortar, coarse aggregate, with the high strength high modulus PVA fiber after Fiber strength for a kind of cement-base composite material strengthened, toughening material forms, it is by short and thin, and the fiber with superperformances such as high-tensile, high limit percentage elongation, high resistance alkalescence is evenly dispersed in a kind of New Building Materials formed in concrete substrate.Owing to adding enhancing, toughness reinforcing PVA fiber, give cement concrete good physical behavior more, Composite is one of main path of Materials, and the technical thought of Composite is over-superimposed effect, namely 1+2>3, PVA fiber reinforcement plays outstanding role in Composite.
Summary of the invention
The object of the invention is to overcome above-mentioned weak point of the prior art and provide a kind of tensile strength, elastic modelling quantity, percentage elongation, draw ratio, interface friction adhesion strength strong, the enhancing of production technology simple concrete, toughness reinforcing PVA fiber production method.
The present invention realizes in the following way:
Concrete strengthens, a production method for toughness reinforcing PVA fiber, it is characterized in that: comprise the following steps:
(1) PVA dissolves: configuring accounting for 0.8 ~ 1.2% crosslinking agent of PVA total polymer weight, 0.05 ~ 0.1% complexing agent, 0.03 ~ 0.08% surfactant, 0.4 ~ 0.6% inorganic acid at dissolving machine and fully to dissolve, temperature controls at 50 ~ 70 DEG C; Then dropped in dissolving machine by the PVA polymer after washing, adopt steam-heated mode, temperature rises to 95 ~ 105 DEG C, lysate is dissolved into the spinning solution that solubility is 13% ~ 28%;
(2) filter together: spinning solution is utilized dissolving machine gear pump carries out constant temperature 100 DEG C, constant 320L/min filters, remove the impurity of PVA polymer self;
(3) deaeration: the mode adopting insulation >=97 DEG C, normal pressure 0.1MPa, by the bubble removal that spinning solution produces in the course of conveying of one filtration step;
(4) two roads filter: by the spinning solution after deaeration, and the filter method of employing constant voltage 0.1Mpa, constant 25ml/min ~ 175ml/min filters, and removes the minute impurities in spinning solution;
(5) spinning: spinning solution enters basic mineral salting liquid through spinnerets ejection and carries out the spinning of wet method semigel, in spinning process, PVA polymer and crosslinking agent carry out network cross-linked in the basic conditions, and with the double diffusion campaign of PVA polymer and inorganic salts, thus form as-spun fibre;
(6) deflector roll is wet stretches: adopt deflector roll to carry out wet stretching to as-spun fibre;
(7) neutralization, solution are cross-linked: the as-spun fibre after wet stretching passes through the inorganic salts mixed liquor containing 1-40g/l acid, carries out network solution cross-linking reaction, carries out the reaction of as-spun fibre dehydrating and curing simultaneously;
(8) damp and hot stretching: adopted by as-spun fibre wet drawing-off bath to carry out damp and hot stretching at the temperature of 85 DEG C ~ 95 DEG C, stretching ratio is between 1-2 times;
(9) wash: by the as-spun fibre after damp and hot stretching by 30 ~ 50 DEG C of water-baths, remove the macerate that as-spun fibre produces from neutralization, solution cross-linking step and damp and hot stretching step, and the crosslinking agent removed on as-spun fibre, the content of crosslinking agent in as-spun fibre controls between 0-1%;
(10) oil: adopted by the as-spun fibre after washing the compound with ionic base to carry out extraction bath, concentration, at 1-10g/l, makes the compound containing ionic base in as-spun fibre; Avoid as-spun fibre to stick together at high operating temperatures, affect as-spun fibre dispersed;
(11) dry: adopt the long drying mode of multistage low temperature to carry out drying the moisture in as-spun fibre the as-spun fibre after oiling, baking temperature segmentation progressively improves, baking temperature, between 100 ~ 200 DEG C, ensures that the moisture content of as-spun fibre is lower than 1%;
(12) preheating: as-spun fibre after drying, under baking storehouse temperature is the condition of 200 DEG C ~ 250 DEG C, brings up to rapidly 210 DEG C ~ 230 DEG C, reaches the vitrification point of as-spun fibre by the surface temperature of as-spun fibre;
(13) xeothermic stretching: xeothermic stretching is carried out to the as-spun fibre after preheating, xeothermic stretching ratio is 2-3 times;
(14) Fiber strength: use non-ionic surface finishing agent to carry out surface treatment to the as-spun fibre after xeothermic stretching; The concentration range 1-10g/l of finishing agent;
(15) dry: dried at the baking storehouse temperature of 100-150 DEG C by the as-spun fibre containing non-ionic surface finishing agent, and make the surface conditioning agent of nonionic penetrate in as-spun fibre, the moisture control of as-spun fibre is below 1%;
(16) reeling: the as-spun fibre after drying is reeled in certain sequence, often roll up weight and be about 300Kg, using in order to cutting off;
(17) cut off, pack: the as-spun fibre of winding is carried out on request cut off and pack.
Described non-ionic surface finishing agent is following one wherein: polyethenoxy ether class, amphenicols, alkyl amine, polyalcohols.
The invention has the advantages that: tensile strength, elastic modelling quantity, percentage elongation, draw ratio, interface friction adhesion strength are strong, and production technology is simple.
Detailed description of the invention
The specific embodiment of the invention is described in detail in detail:
A kind of concrete strengthens, the production method of toughness reinforcing PVA fiber, comprise the following steps: (1) PVA dissolves: configuring accounting for 0.8 ~ 1.2% crosslinking agent of PVA total polymer weight, 0.05 ~ 0.1% complexing agent, 0.03 ~ 0.08% surfactant, 0.4 ~ 0.6% inorganic acid at dissolving machine and fully to dissolve, temperature controls at 50 ~ 70 DEG C; Then dropped in dissolving machine by the PVA polymer after washing, adopt steam-heated mode, temperature rises to 95 ~ 105 DEG C, lysate is dissolved into the spinning solution that solubility is 13% ~ 28%; (2) filter together: spinning solution is utilized dissolving machine gear pump carries out constant temperature 100 DEG C, constant 320L/min filters, remove the impurity of PVA polymer self; (3) deaeration: the mode adopting insulation >=97 DEG C, normal pressure 0.1MPa, by the bubble removal that spinning solution produces in the course of conveying of one filtration step; (4) two roads filter: by the spinning solution after deaeration, and the filter method of employing constant voltage 0.1Mpa, constant 25ml/min ~ 175ml/min filters, and removes the minute impurities in spinning solution; (5) spinning: spinning solution enters basic mineral salting liquid through spinnerets ejection and carries out the spinning of wet method semigel, in spinning process, PVA polymer and crosslinking agent carry out network cross-linked in the basic conditions, and with the double diffusion campaign of PVA polymer and inorganic salts, thus form as-spun fibre; (6) deflector roll is wet stretches: adopt deflector roll to carry out wet stretching to as-spun fibre; (7) neutralization, solution are cross-linked: the as-spun fibre after wet stretching passes through the inorganic salts mixed liquor containing 1-40g/l acid, carries out network solution cross-linking reaction, carries out the reaction of as-spun fibre dehydrating and curing simultaneously; (8) damp and hot stretching: adopted by as-spun fibre wet drawing-off bath to carry out damp and hot stretching at the temperature of 85 DEG C ~ 95 DEG C, stretching ratio is between 1-2 times; (9) wash: by the as-spun fibre after damp and hot stretching by 30 ~ 50 DEG C of water-baths, remove the macerate that as-spun fibre produces from neutralization, solution cross-linking step and damp and hot stretching step, and the crosslinking agent removed on as-spun fibre, the content of crosslinking agent in as-spun fibre controls between 0-1%; (10) oil: adopted by the as-spun fibre after washing the compound with ionic base to carry out extraction bath, concentration, at 1-10g/l, makes the compound containing ionic base in as-spun fibre; Avoid as-spun fibre to stick together at high operating temperatures, affect as-spun fibre dispersed; (11) dry: adopt the long drying mode of multistage low temperature to carry out drying the moisture in as-spun fibre the as-spun fibre after oiling, baking temperature segmentation progressively improves, baking temperature, between 100 ~ 200 DEG C, ensures that the moisture content of as-spun fibre is lower than 1%; (12) preheating: as-spun fibre after drying, under baking storehouse temperature is the condition of 200 DEG C ~ 250 DEG C, brings up to rapidly 210 DEG C ~ 230 DEG C, reaches the vitrification point of as-spun fibre by the surface temperature of as-spun fibre; (13) xeothermic stretching: xeothermic stretching is carried out to the as-spun fibre after preheating, xeothermic stretching ratio is 2-3 times; (14) Fiber strength: use non-ionic surface finishing agent to carry out surface treatment to the as-spun fibre after xeothermic stretching; The concentration range 1-10g/l of finishing agent; (15) dry: dried at the baking storehouse temperature of 100-150 DEG C by the as-spun fibre containing non-ionic surface finishing agent, and make the surface conditioning agent of nonionic penetrate in as-spun fibre, the moisture control of as-spun fibre is below 1%; (16) reeling: the as-spun fibre after drying is reeled in certain sequence, often roll up weight and be about 300Kg, using in order to cutting off; (17) cut off, pack: the as-spun fibre of winding is carried out on request cut off and pack.
Non-ionic surface finishing agent of the present invention is following one wherein: polyethenoxy ether class, amphenicols, alkyl amine, polyalcohols.
Embodiment 1
The PVA polymer 900 ~ 1000Kg of viscosity average polymerization degree 1700, saponification degree 97 Mole percent is added in the aqueous mixtures containing 9Kg crosslinking agent, 0.9Kg complexing agent, 4.5L inorganic acid, 0.5Kg surfactant, dissolve under 100-105 DEG C of dissolving machine, obtain the spinning solution that solubility reaches 16%, be the spinnerets of 0.10mm, hole count 16000 by diameter by the spinning solution obtained, in the fixation bath that the NaOH/NaSO4 proportion 1.280 of liquid temperature 45 DEG C is formed, carry out the spinning of wet method semigel; The as-spun fibre obtained is immersed in the neutralization bath of H2SO4/NaSO4 composition proportion 1.300 and is cured reaction, then with in and bathe and form during temperature 90 DEG C is bathed the damp and hot stretching implementing 1.6 times equally, thereafter wash in 40 DEG C of water-baths, remove the crosslinking agent in the acid of unnecessary as-spun fibre attachment and polymer.Upper oil guard is carried out in the oil bath as-spun fibre obtained being immersed in 8-10g/l, as-spun fibre is evenly oiled, in baking storehouse, multistage oven dry is carried out to as-spun fibre by the temperature of 100 ~ 200 DEG C, then as-spun fibre is dried in storehouse at 200 ~ 230 DEG C and carry out xeothermic stretching, make always to draw multiple to reach 12 times, obtain spinning precursor; Spinning precursor is immersed in the nonionic process bath containing 3-5g/l, carries out the surface treatment of spinning precursor, then at 100-150 DEG C of temperature, carry out multistage oven dry, and reel, obtained concrete enhancing, toughness reinforcing PVA fiber; The physical property of the fiber obtained is as follows: single fiber diameter 15 μm, fibre tensile strength 1534MPa, fiber isotropic modulus 37.7GPa, elongate fiber rate 6.5%, alkali resistance 100%, fibre frictoin adhesion strength 4.0MPa, meets the requirement of ECC to PVA fiber quality.
Embodiment 2
The PVA polymer 900 ~ 1000Kg of viscosity average polymerization degree 2000, saponification degree 97 Mole percent is added in the aqueous mixtures containing 10Kg crosslinking agent, 0.9Kg complexing agent, 4.8L inorganic acid, 0.5Kg surfactant, dissolve under 100-105 DEG C of dissolving machine, obtain the spinning solution that solubility reaches 15%, be the spinnerets of 0.11mm, hole count 2000 by diameter by the spinning solution obtained, in the fixation bath that the NaOH/NaSO4 proportion 1.280 of liquid temperature 45 DEG C is formed, carry out the spinning of wet method semigel; The as-spun fibre obtained is immersed in the neutralization bath of H2SO4/NaSO4 composition proportion 1.300 and is cured reaction, then with in and bathe and form during temperature 90 DEG C is bathed the damp and hot stretching implementing 1.6 times equally, thereafter wash in 40 DEG C of water-baths, remove the crosslinking agent in the acid of unnecessary as-spun fibre attachment and polymer.Upper oil guard is carried out in the oil bath as-spun fibre obtained being immersed in 8-10g/l, as-spun fibre is evenly oiled, in baking storehouse, multistage oven dry is carried out to as-spun fibre by the temperature of 100 ~ 200 DEG C, then as-spun fibre is dried in storehouse at 200 ~ 230 DEG C and carry out xeothermic stretching, make always to draw multiple to reach 12 times, obtain spinning precursor; Spinning precursor is immersed in the nonionic process bath containing 3-5g/l, carries out the surface treatment of spinning precursor, then at 100-150 DEG C of temperature, carry out multistage oven dry, and reel, obtained concrete enhancing, toughness reinforcing PVA fiber; The physical property of the fiber obtained is as follows: single fiber diameter 38 μm, fibre tensile strength 1365MPa, fiber isotropic modulus 36.4GPa, elongate fiber rate 6.5%, alkali resistance 100%, fibre frictoin adhesion strength 3.50MPa, meets the requirement of ECC to PVA fiber quality.
Claims (1)
1. a production method for concrete enhancing, toughness reinforcing PVA fiber, is characterized in that: comprise the following steps:
(1) PVA dissolves: configuring accounting for 0.8 ~ 1.2% crosslinking agent of PVA total polymer weight, 0.05 ~ 0.1% complexing agent, 0.03 ~ 0.08% surfactant, 0.4 ~ 0.6% inorganic acid at dissolving machine and fully to dissolve, temperature controls at 50 ~ 70 DEG C; Then dropped in dissolving machine by the PVA polymer after washing, adopt steam-heated mode, temperature rises to 95 ~ 105 DEG C, lysate is dissolved into the spinning solution that concentration is 13% ~ 28%;
(2) filter together: spinning solution is utilized dissolving machine gear pump carries out constant temperature 100 DEG C, constant 320L/min filters, remove the impurity of PVA polymer self;
(3) deaeration: the mode adopting insulation >=97 DEG C, normal pressure 0.1MPa, by the bubble removal that spinning solution produces in the course of conveying of one filtration step;
(4) two roads filter: by the spinning solution after deaeration, and the filter method of employing constant voltage 0.1MPa, constant 25ml/min ~ 175ml/min filters, and removes the minute impurities in spinning solution;
(5) spinning: spinning solution enters basic mineral salting liquid through spinnerets ejection and carries out the spinning of wet method semigel, in spinning process, PVA polymer and crosslinking agent carry out network cross-linked in the basic conditions, and with the double diffusion campaign of PVA polymer and inorganic salts, thus form as-spun fibre;
(6) deflector roll is wet stretches: adopt deflector roll to carry out wet stretching to as-spun fibre;
(7) neutralization, solution are cross-linked: the as-spun fibre after wet stretching passes through the inorganic salts mixed liquor containing 1-40g/l acid, carries out network solution cross-linking reaction, carries out the reaction of as-spun fibre dehydrating and curing simultaneously;
(8) damp and hot stretching: adopted by as-spun fibre wet drawing-off bath to carry out damp and hot stretching at the temperature of 85 DEG C ~ 95 DEG C, stretching ratio is between 1-2 times;
(9) wash: by the as-spun fibre after damp and hot stretching by 30 ~ 50 DEG C of water-baths, remove the macerate that as-spun fibre produces from neutralization, solution cross-linking step and damp and hot stretching step, and the crosslinking agent removed on as-spun fibre, the content of crosslinking agent in as-spun fibre controls between 0-1%;
(10) oil: adopted by the as-spun fibre after washing the compound with ionic base to carry out extraction bath, concentration, at 1-10g/l, makes the compound containing ionic base in as-spun fibre; Avoid as-spun fibre to stick together at high operating temperatures, affect as-spun fibre dispersed;
(11) dry: to adopt the long drying mode of multistage low temperature to carry out drying the moisture in as-spun fibre the as-spun fibre after oiling, baking temperature segmentation progressively improves, baking temperature, between 100 ~ 200 DEG C, ensures that the moisture content of as-spun fibre is lower than 1%;
(12) preheating: as-spun fibre after drying, under baking storehouse temperature is the condition of 200 DEG C ~ 250 DEG C, brings up to rapidly 210 DEG C ~ 230 DEG C, reaches the vitrification point of as-spun fibre by the surface temperature of as-spun fibre;
(13) xeothermic stretching: xeothermic stretching is carried out to the as-spun fibre after preheating, xeothermic stretching ratio is 2-3 times;
(14) Fiber strength: use non-ionic surface finishing agent to carry out surface treatment to the as-spun fibre after xeothermic stretching; The concentration range 1-10g/l of finishing agent;
(15) dry: dried at the baking storehouse temperature of 100-150 DEG C by the as-spun fibre containing non-ionic surface finishing agent, and make the surface conditioning agent of nonionic penetrate in as-spun fibre, the moisture control of as-spun fibre is below 1%;
(16) reeling: the as-spun fibre after drying is reeled in certain sequence, often roll up weight and be about 300Kg, using in order to cutting off;
(17) cut off, pack: the as-spun fibre of winding is carried out on request cut off and pack.
2. the production method of a kind of concrete enhancing according to claim 1, toughness reinforcing PVA fiber, is characterized in that: described non-ionic surface finishing agent is following one wherein: polyethenoxy ether class, amphenicols, alkyl amine, polyalcohols.
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| CN107269295A (en) * | 2017-06-29 | 2017-10-20 | 昆明理工大学 | A kind of PVA ECC set lining structures and construction method |
| CN110983846A (en) * | 2019-12-19 | 2020-04-10 | 蚌埠产品质量监督检验研究院 | Preparation method of sisal cellulose whisker, non-woven fabric for filter and preparation method |
| CN114318558B (en) * | 2021-12-24 | 2022-12-16 | 桐乡市中益化纤有限公司 | FDY fiber subjected to online alkali reduction treatment and preparation method thereof |
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| JPH05247720A (en) * | 1992-03-07 | 1993-09-24 | Nichibi:Kk | Water-soluble colored polyvinyl alcohol yarn and its production |
| CN1081686C (en) * | 1998-04-14 | 2002-03-27 | 中国石油化工总公司 | Wet PVA-crosslinking spinning technology |
| CN101177800B (en) * | 2006-11-06 | 2010-08-11 | 湖南省湘维有限公司 | Water-soluble polyvinyl alcohol fibre and preparation technique thereof |
| CN103031611B (en) * | 2011-09-30 | 2016-01-20 | 中国石油化工集团公司 | A kind of vinal and its preparation method and application |
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